CN110514498B - Method for preparing metal expanded couple by centrifugal method - Google Patents
Method for preparing metal expanded couple by centrifugal method Download PDFInfo
- Publication number
- CN110514498B CN110514498B CN201910859902.3A CN201910859902A CN110514498B CN 110514498 B CN110514498 B CN 110514498B CN 201910859902 A CN201910859902 A CN 201910859902A CN 110514498 B CN110514498 B CN 110514498B
- Authority
- CN
- China
- Prior art keywords
- quartz tube
- metal
- motor
- couple
- diffusion
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
Landscapes
- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Sampling And Sample Adjustment (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
The invention discloses a method for preparing a metal diffusion couple by a centrifugal method, which mainly prepares a diffusion couple (shown as an A \ B couple) consisting of metal (shown as A) and metal (shown as B), and can prepare solid metal or an A \ B couple consisting of solid-liquid metal according to needs. A pair of A, B wires or rods of equal length and diameter were placed in a quartz tube, evacuated to a high vacuum and sealed with an oxyhydrogen flame. The middle position of the quartz tube in the length direction is vertically fixed on a long metal molybdenum rod, the molybdenum rod is connected with a motor, the quartz tube is placed in a resistance furnace, the quartz tube rotates at a high speed in the furnace, so that the metal A and the metal B are in close contact with each other under the action of centrifugal force to form an A \ B diffusion couple, after the motor reaches a set rotating speed, the rotating speed is gradually reduced until the motor stops, then the quartz tube is taken out for air cooling or quenching cooling, and finally the quartz tube is broken and the prepared diffusion couple is taken out.
Description
Technical Field
The invention relates to a preparation method of a metal diffusion couple, belonging to the field of metal material research. The method is mainly used in the fields of phase diagram measurement, thermodynamic and kinetic performance test of metal materials, brazing materials, high-temperature structural materials and the like.
Background
Diffusion couples were first introduced in the research of materials, metallurgical science. The general diffusion couple refers to a sample formed by metallurgically bonding two materials together after diffusion, and the diffusion is carried out in the direction vertical to the metallurgic bonding surface, so that the continuous transition of the components from the material 1 to the material 2 with a certain thickness is formed, or a phase interface is formed, and the thickness of the transition layer can meet the requirement of measuring the component distribution by using an electronic probe. Although the transition layer or the phase interface is a two-dimensional surface in a macroscopic view, two sides of the interface are considered to be in a local equilibrium state based on the local equilibrium principle. The early diffusion couple is mostly binary, and the later diffusion couple and the quaternary diffusion couple appear along with the development of a phase diagram testing technology, and particularly, the diffusion multi-element section appears along with the rapid development of a high-throughput preparation technology in material genome engineering in 2012.
The methods for preparing the diffusion couples are classified according to the states of the components of the diffusion couples, and can be classified into a solid/solid diffusion method, a solid/liquid diffusion method and a solid/gas diffusion method. The preparation method of the diffusion couple can be divided into a binary diffusion couple, a ternary diffusion couple, a quaternary diffusion couple and a higher diffusion couple. The preparation of the binary diffusion couple generally comprises a binding method, a riveting method, a rolling method, a solid-liquid dipping method and the like. Common methods for preparing ternary diffusion couples include a 'pin' bonding method, a 'rivet method', a 'fire layer method' and the like. The four-element and higher-element diffusion couple preparation is usually combined by the above methods. The main methods for preparing the diffusion couple are briefly described below.
Binding method: grinding the surfaces to be diffused of the two components to be polished into mirror surfaces, then superposing the two components to make the two mirror surfaces contact with each other, firmly binding the two components by molybdenum wires, placing the two components into a quartz tube, vacuumizing, sealing and preparing a diffusion couple.
The rolling method comprises the following steps: cutting two components to be diffused into small blocks, grinding and polishing the surface to be diffused into a mirror surface, slowly applying pressure to the two components by using a hydraulic press to ensure that the two components are tightly attached together under the action of external pressure, then putting the attached sample into a quartz tube, vacuumizing and sealing to prepare the diffusion couple.
Evaporation method: the evaporation method is that the components A and B to be diffused are placed in evaporation equipment, and a layered evaporation method is adopted under a certain temperature and vacuum environment, and the sequence of evaporation of the components to be diffused is controlled by a control valve, so that the components are sequentially evaporated on a substrate to prepare a diffusion couple.
Deposition method: the deposition method is mainly used for preparing a film-type diffusion couple, and the main modes are chemical or electrochemical deposition and vapor deposition. The electrochemical deposition is that in a solution containing metal ions, the metal ions obtain electrons at a cathode under the action of an electric field, and are reduced, so that the metal ions are deposited on the metal surface of the cathode. The vapor deposition technique is to deposit gaseous or vapor chemical substances directly or via chemical reaction into a solid deposition layer in a deposition chamber by means of plasma excitation or equal heating.
Diffusion bonding (vacuum thermocompression): the vacuum hot pressing method is to polish the surface of the material to be diffused by using sand paper to make the surface smooth and clean and have certain roughness, to clean the surface, to remove surface oxides and grease, to apply pressure to the components to be diffused under certain temperature and vacuum condition, to connect the components to be diffused together by the diffusion between atoms, to prepare the diffusion couple sample.
Powder pressing method: making one group of elements to be diffused into powder, making the other group of elements into rod-like elements, utilizing special mould to coat the rod-like elements with the powder group of elements, pressing them into block form, placing them into quartz tube, vacuum-pumping and sealing so as to obtain the invented diffusion couple.
The clamping method comprises the following steps: the clamp method is that the interface to be diffused of different component materials is grinded into mirror surface by the method of grinding metallographic structure, and is cleaned, so that the two interfaces are jointed, the two grinded interfaces to be diffused are ensured to be straight, the two interfaces are contacted without seam and light transmission, impurities irrelevant to the experiment are prevented from entering the interfaces, the interface is placed in the middle position of the clamp and is fixed by the clamp, then the sample is placed in a quartz tube, and the quartz tube is vacuumized and sealed to prepare the diffusion couple sample.
The riveting method comprises the following steps: the riveting method is characterized in that two materials with larger difference of thermal expansion coefficients are used, wherein the material with the smaller thermal expansion coefficient is used as a base material, a through hole is processed in the middle of the base material, the material with the larger thermal expansion coefficient is processed into a cone with certain taper, the surface of the cone and the surface of the through hole are polished by abrasive paper, and an oxidation film is removed. And (3) quickly pressing the cone into the processed through hole from the small end through external pressure, so as to realize interference fit between the rivet and the base body and prepare a diffusion couple sample.
In the existing preparation methods of the diffusion couple, no method and report for preparing the diffusion couple by using the centrifugal force or the centripetal force generated when the material rotates at high speed are found.
Disclosure of Invention
The method for preparing a metal diffusion couple by a centrifugal method of the present invention mainly prepares a diffusion couple (shown as an A/B couple) composed of a metal (shown as A) and a metal (shown as B), and can prepare a solid metal or an A/B couple composed of a solid metal as required. The preparation method comprises the following steps:
firstly, a pair of A, B metal wires or rods with the same length and the same diameter are put into a horizontally-placed quartz tube with a bottom seal with a slightly larger inner diameter according to the sequence of A-B-B-A;
then, after the quartz tube is pumped to high vacuum and filled with high-purity argon for 4 times by adopting vacuum equipment, keeping a certain vacuum degree, and sealing the tube by adopting oxyhydrogen flame;
then, vertically fixing the middle position of the quartz tube in the length direction on a long metal molybdenum rod, and connecting the molybdenum rod with a motor; and then horizontally placing the quartz tube into a vertical resistance furnace, and ensuring that the metal rods and wires at two ends of the quartz tube are as follows: a is arranged outside and B is arranged inside;
then, the long metal molybdenum rod is transmitted out through a hole in the center of the top of the electric furnace and is well connected with a motor shaft; then the electric furnace is heated to a set temperature, the motor is started to enable the quartz tube to rotate at a high speed in the furnace, the A metal wire or rod and the B metal wire or rod are in close contact with each other under the action of centrifugal force to form an A/B diffusion couple, after the motor reaches a set rotating speed and is kept for a certain time,
and gradually reducing the rotating speed until the quartz tube is stopped, taking out the quartz tube for air cooling or quenching cooling, and breaking the diffusion couple prepared by taking out the quartz tube.
And then, the prepared diffusion couple can be further subjected to diffusion treatment at the temperature required for experiments, so that corresponding experiments and analysis are carried out.
Detailed Description
The specific processing method of the preparation process is described below as above.
The first embodiment is as follows:
(1) firstly, a pair of metal rods A (metal Al) and B (metal Cu) with the diameters of both 10mm and 4mm is put into a horizontally-placed quartz tube with a bottom seal with the inner diameter of 4.1mm and the wall thickness of 1mm according to the sequence of A-B-B-A;
(2) then, a vacuum device is adopted to pump the quartz tube to high vacuum and fill high-purity argon for 4 times, the condition of 0.8 atmospheric pressure is kept, and then oxyhydrogen flame is adopted to seal the tube;
(3) then, vertically fixing the middle position of the quartz tube in the length direction on a long metal molybdenum rod, and connecting the molybdenum rod with a motor; and then horizontally placing the quartz tube into a vertical resistance furnace, and ensuring that the metal rods at two ends of the quartz tube are as follows: a is arranged outside and B is arranged inside;
(4) then, the long metal molybdenum rod is transmitted out through a hole in the center of the top of the electric furnace and is well connected with a motor shaft; then the electric furnace is heated to 400 ℃, a motor is started to enable the quartz tube to rotate at a high speed in the furnace, so that the metal A and the metal B are in close contact with each other under the action of centrifugal force to form an A/B diffusion couple, after the motor reaches a set rotating speed (120 revolutions per minute), the motor is kept for 1 hour,
(5) and gradually reducing the rotating speed until the quartz tube is stopped, taking out the quartz tube for air cooling or quenching cooling, and breaking the Al/Cu diffusion couple prepared by taking out the quartz tube.
Example two:
(1) firstly, a pair of A (metal Sn) metal rods with the length of 5mm and the diameter of 10mm and a pair of B (metal Cu) metal rods with the diameter of 10mm are put into a horizontally-placed quartz tube with a bottom seal with the inner diameter of 10.2mm and the wall thickness of 1mm according to the sequence of A-B-B-A;
(2) then, after the quartz tube is pumped to high vacuum and filled with high-purity argon for 4 times by adopting vacuum equipment, sealing the tube by adopting oxyhydrogen flame under the condition of 0.9 atmospheric pressure; (ii) a
(3) Then, vertically fixing the middle position of the quartz tube in the length direction on a long metal molybdenum rod, and connecting the molybdenum rod with a motor; and then horizontally placing the quartz tube into a vertical resistance furnace, and ensuring that the metal rods at two ends of the quartz tube are as follows: a is arranged outside and B is arranged inside;
(4) then, the long metal molybdenum rod is transmitted out through a hole in the center of the top of the electric furnace and is well connected with a motor shaft; then the electric furnace is heated to 200 ℃, then the motor is started to enable the quartz tube to rotate at high speed in the furnace, the metal A and the metal B are closely contacted together to form an A/B diffusion couple under the action of centrifugal force, after the motor reaches a set rotating speed (60 revolutions per minute), the motor is kept for 30 minutes,
(5) and gradually reducing the rotating speed until the quartz tube is stopped, taking out the quartz tube for air cooling or quenching and cooling, and breaking the Sn/Cu diffusion couple prepared by taking out the quartz tube.
Claims (2)
1. A method for preparing metal diffusion couples by a centrifugal method is characterized by comprising the following process steps:
(1) firstly, a pair of A, B metal wires or rods with the same length and the same diameter are put into a horizontally-placed quartz tube with a bottom seal with a slightly larger inner diameter according to the sequence of A-B-B-A;
(2) then, after the quartz tube is pumped to high vacuum and filled with high-purity argon for 4 times by adopting vacuum equipment, keeping a certain vacuum degree, and sealing the tube by adopting oxyhydrogen flame;
(3) then, vertically fixing the middle position of the quartz tube in the length direction on a long metal molybdenum rod, and connecting the molybdenum rod with a motor; and then horizontally placing the quartz tube into a vertical resistance furnace, and ensuring that the metal wires or rods at two ends of the quartz tube are as follows: a is arranged outside and B is arranged inside;
(4) then, the long metal molybdenum rod is transmitted out through a hole in the center of the top of the electric furnace and is well connected with a motor shaft; then, after the electric furnace is heated to a set temperature, a motor is started to enable the quartz tube to rotate at a high speed in the furnace, so that the A metal wire or rod and the B metal wire or rod are in close contact with each other under the action of centrifugal force to form an A/B diffusion couple, and the motor is kept for a certain time after reaching a set rotating speed;
(5) gradually reducing the rotating speed until the quartz tube is stopped, taking out the quartz tube for air cooling or quenching and cooling, and breaking the diffusion couple prepared by taking out the quartz tube.
2. A method for preparing metal diffusion couples by a centrifugal method is characterized by comprising the following process steps:
(1) firstly, a pair of metal rods A, namely metal Al and B, namely metal Cu, which are 10mm in diameter and 4mm in diameter are put into a horizontally-placed quartz tube with a bottom seal with the inner diameter of 4.1mm and the wall thickness of 1mm according to the sequence of A-B-B-A;
(2) then, a vacuum device is adopted to pump the quartz tube to high vacuum and fill high-purity argon for 4 times, the condition of 0.8 atmospheric pressure is kept, and then oxyhydrogen flame is adopted to seal the tube;
(3) then, vertically fixing the middle position of the quartz tube in the length direction on a long metal molybdenum rod, and connecting the molybdenum rod with a motor; and then horizontally placing the quartz tube into a vertical resistance furnace, and ensuring that the metal rods at two ends of the quartz tube are as follows: a is arranged outside and B is arranged inside;
(4) then, the long metal molybdenum rod is transmitted out through a hole in the center of the top of the electric furnace and is well connected with a motor shaft; then, after the electric furnace is heated to 400 ℃, starting a motor to enable the quartz tube to rotate at a high speed in the furnace, enabling the metal A and the metal B to be in close contact with each other under the action of centrifugal force to form an A/B diffusion couple, and keeping the motor for 1 hour after the motor reaches a set rotating speed which is 120 revolutions per minute;
(5) gradually reducing the rotating speed until the quartz tube is stopped, taking out the quartz tube for air cooling or quenching and cooling, and breaking the Al/Cu diffusion couple prepared by taking out the quartz tube.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910859902.3A CN110514498B (en) | 2019-09-11 | 2019-09-11 | Method for preparing metal expanded couple by centrifugal method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910859902.3A CN110514498B (en) | 2019-09-11 | 2019-09-11 | Method for preparing metal expanded couple by centrifugal method |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN110514498A CN110514498A (en) | 2019-11-29 |
| CN110514498B true CN110514498B (en) | 2021-11-19 |
Family
ID=68630721
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201910859902.3A Active CN110514498B (en) | 2019-09-11 | 2019-09-11 | Method for preparing metal expanded couple by centrifugal method |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN110514498B (en) |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112557136B (en) * | 2020-11-16 | 2023-05-23 | 上海大学 | Multi-element alloy diffusion couple device and multi-element alloy diffusion coefficient determination experiment method |
| CN113189127B (en) * | 2021-04-13 | 2023-01-24 | 昆明贵金属研究所 | Method for preparing high-melting-point metal ternary diffusion couple |
| CN113899603A (en) * | 2021-09-16 | 2022-01-07 | 贵研铂业股份有限公司 | Method for preparing diffusion couple by hole type rolling mill |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101892444A (en) * | 2010-07-09 | 2010-11-24 | 燕山大学 | Method for preparing Ti50-Fe25-Ni25 ternary amorphous alloy |
| CN106442224A (en) * | 2014-09-17 | 2017-02-22 | 合肥工业大学 | Method for preparing metal melt diffusion sample based on thin-layer diffusion model |
| CN206134069U (en) * | 2016-07-28 | 2017-04-26 | 宋笑尘 | Al and even preparation facilities of cu reaction |
-
2019
- 2019-09-11 CN CN201910859902.3A patent/CN110514498B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101892444A (en) * | 2010-07-09 | 2010-11-24 | 燕山大学 | Method for preparing Ti50-Fe25-Ni25 ternary amorphous alloy |
| CN106442224A (en) * | 2014-09-17 | 2017-02-22 | 合肥工业大学 | Method for preparing metal melt diffusion sample based on thin-layer diffusion model |
| CN206134069U (en) * | 2016-07-28 | 2017-04-26 | 宋笑尘 | Al and even preparation facilities of cu reaction |
Non-Patent Citations (1)
| Title |
|---|
| 镍基高温合金HIP扩散连接的组织和性能;闫来成等;《钢铁研究学报》;全文 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN110514498A (en) | 2019-11-29 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN110514498B (en) | Method for preparing metal expanded couple by centrifugal method | |
| CN110608931B (en) | High-flux preparation method for preparing metal diffusion couples with large melting point difference | |
| US9999947B2 (en) | Method for repairing heaters and chucks used in semiconductor processing | |
| JPH0873280A (en) | Joined body and its production | |
| CN110340331B (en) | Method for efficiently preparing ternary diffusion couple | |
| WO2016109793A1 (en) | High temperature method for joining materials and devices utilizing same | |
| CN102189261A (en) | Densification method of porous workpiece | |
| CN107022733B (en) | Molten salt thermal diffusion treatment equipment and application thereof | |
| CN111151763A (en) | Preparation method of tungsten-titanium alloy target material | |
| CN110280741A (en) | A kind of preparation method of Sn-Bi bianry alloy diffusion couple | |
| JP7076984B2 (en) | How to repair defects in high temperature parts of turbomachinery through a hybrid hot hydrostatic press (HIP) process | |
| CN103938009A (en) | Method of preparing porous foam alloy and removing pore forming material sodium metaaluminate | |
| US10926323B2 (en) | Systems and methods for counter gravity casting for bulk amorphous alloys | |
| JPH10287483A (en) | Air-tight part and its production | |
| CN110595955A (en) | Method for preparing easily oxidized metal diffusion couple | |
| Hausner et al. | Brazing of metal and ceramic joints | |
| CN110983148B (en) | Additive manufacturing method and product of high-entropy alloy based on precious metal material | |
| Matsuura et al. | In-situ joining of nickel monoaluminide to iron by reactive sintering | |
| Harpster et al. | Field-assisted bonding of glass to Si-Au eutectic solder for packaging applications | |
| CN103193507B (en) | Method for improving wettability of metal to SiC ceramic | |
| CN104715994B (en) | Inductive type plasma process chamber and its anticorrosive insulated window and manufacture method | |
| JP3941542B2 (en) | Hermetic bonding structure of ceramics and metal and apparatus parts having the structure | |
| Hu et al. | Fractal pattern formation in anodic bonding of Pyrex glass/Al/Si | |
| CN112935509B (en) | Large-size titanium alloy bar processing device | |
| CN106695047B (en) | A kind of SiO2The method of ceramic matric composite surface active assistant brazing |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20230628 Address after: No. 988, Keji Road, high tech Industrial Development Zone, Kunming, Yunnan 650000 Patentee after: Yunnan Precious Metals Laboratory Co.,Ltd. Address before: No. 988, Keji Road, high tech Development Zone, Wuhua District, Kunming, Yunnan 650000 (Kunming Precious Metals Research Institute) Patentee before: Sino-Platinum Metals Co.,Ltd. |
|
| TR01 | Transfer of patent right |